In the present study, a polar-embedded reversed-phase liquid chromatographic stationary phase that contained internal sulfone groups was prepared. The synthesis involved the "thiol-ene" click chemistry between the vinyl functionalized silica and 1-octadecanethiol, followed by the oxidization of sulfide to sulfone groups. The resulting material simultaneously possessed the alkyl chain, i.e. C18, and the internal sulfone groups. Elemental analysis demonstrates that the element contents of the C18/sulfone silica were C 8.94%, H 1.87% and S 0.66%. Chromatographic evaluations indicate that the C18/sulfone stationary phase exhibited a little less retention than the C18/sulfide one. A comparable chromatographic performance of neutral analytes was obtained on these two columns, but much better chromatographic performance in the case of basic and acid analytes was obtained on C18/sulfone stationary phase with additional features such as lower silanol activity, better stability (stable working conditions of pH 1.0-10.0), and better compatibility with 100% aqueous mobile phases. The batch-to-batch reproducibility was acceptable (the RSDs of retention times for the probes were no higher than 1.73%), demonstrating the suitability of the applied synthetic strategy for the new stationary phase. The C18/sulfone is a promising polar-embedded RPLC stationary phase.
Download full-text PDF |
Source |
---|---|
http://dx.doi.org/10.1002/jssc.201700751 | DOI Listing |
Org Chem Front
December 2024
Department of Chemistry, University of Basel St Johanns-Ring 19 Basel 4056 Switzerland https://www.chemie1.unibas.ch/Bmayor/.
This work explores the use of a cross-shaped organic framework that is used as a template for the investigation of multi-functionalized chromophores. We report the design and synthesis of a universal cross-shaped building block bearing two bromines and two iodines on its peripheral positions. The template can be synthesized on a gram scale in a five-step reaction comprising an oxidative homo-coupling macro-cyclization.
View Article and Find Full Text PDFJ Sep Sci
December 2024
College of Chemistry and Chemical Engineering, Yunnan Normal University, Kunming, China.
Chiral macrocycles have emerged as attractive media for chromatographic enantioseparation due to their excellent host-guest recognition properties. In this study, a new chiral stationary phase (CSP) based on 1,1'-binaphthyl chiral polyimine macrocycle (CPM) was reported. The CPM was synthesized by one-step aldehyde-amine condensation of (S)-2,2'-dihydroxy-[1,1'-binaphthalene]-3,3'-dicarboxaldehyde with 1,2-phenylenediamine and bonded on thiolated silica via the thiol-ene click reaction to afford the CSP.
View Article and Find Full Text PDFAnal Chem
December 2024
Department of Chemistry, National Demonstration Centre for Experimental Chemistry Education, Yanbian University, Yanji City 133002, Jilin Province, China.
Generally, the traditional stationary phase for liquid chromatography is the key part, but with an in situ immutable property, leading to many separation limitations. Based on the former exploration of photosensitive gas chromatography, we successfully prepared a photosensitive monolithic capillary silica column with high light transmission, taking advantage of the reversible cis-trans isomerism of azobenzene. And the cis-trans isomerism has launched an effective, reversible, and precise control on the liquid chromatographic retention behavior just by photoinduction according to the theoretical basis of a good correlation between photoinduction time, -azobenzene ratio, and chromatographic retention factor () ( > 0.
View Article and Find Full Text PDFMicrobiol Res
December 2024
Commonwealth Scientific and Industrial Research Organisation (CSIRO), Agriculture and Food, Acton, ACT, Australia; Commonwealth Scientific and Industrial Research Organisation (CSIRO), Advanced Engineering Biology Future Science Platform, Acton, ACT, Australia; Commonwealth Scientific and Industrial Research Organisation (CSIRO), Microbiomes for One Systems Health Future Science Platform, Acton, ACT, Australia.
The use of multi-omic approaches has significantly advanced the exploration of microbial traits, leading to the discovery of new bioactive compounds and their mechanisms of action. Streptomyces sp. MH71 is known for its antifungal properties with potential for use in crop protection.
View Article and Find Full Text PDFJ Sep Sci
December 2024
Institute of Pharmaceutical Sciences, Pharmaceutical (Bio-)Analysis, University of Tübingen, Tübingen, Germany.
The present work reports on the preparation, characterization, and evaluation of a set of novel triphenyl-modified silica-based stationary phases without and with embedded ion-exchange sites for mixed-mode liquid chromatography. The three synthesized triphenyl phases differed in additionally incorporated ion-exchange sites. In one embodiment, allyltriphenylsilane was bonded to thiol-modified silica by thiol-ene click reaction, leading to particles with no ion-exchange sites.
View Article and Find Full Text PDFEnter search terms and have AI summaries delivered each week - change queries or unsubscribe any time!